EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/04src0993

Report generated Nov 19, 2004; 11:07:19

Unit cell

2616 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)11.4444 +/- 0.0002
b (Angstrom)5.95180 +/- 0.00010
c (Angstrom)15.6233 +/- 0.0002
alpha (°) 90.000
beta (°)100.1475 +/- 0.0010
gamma (°) 90.000
Volume (A**3)1047.53 +/- 0.03
Mosaicity (°)0.5430 +/- 0.0010

Data collection

Summary

Total number of images collected441
Total exposure time16.2 minutes
Data collection exposure time16.0 minutes
Data collection wall-clock time50.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f222222.0° phi1.000°2 secondsYes
data collections02f108108.0° omega1.000°2 secondsYes
data collections03f103103.0° omega1.000°2 secondsYes
Phi/Chii01f - i08f81 seconds

Scalepack Scaling

Deleted observations

Rejected 153
Zero sigma or profile test   4
Overload or incomplete profile 850
Sigma cutoff   4

Final Data Set

Scale factor range8.19-13.70
Number of 'full' reflections  4951
Number of 'partial' reflections 11989
Total number of integrated reflections 16086
Total number of unique reflections  2635
Data completeness  98.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  320.9
Average Sigma(I)    6.0
Overall R-merge (linear)  0.037

Sadabs Results

Parameter refinement on 13578 reflections reduced R(int) from 0.1024 to 0.0351

Before rejection, 16309 reflections total and 2642 unique

After rejection, 16027 reflections total and 2635 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0351   0.676 - 0.905   0.931 - 1.132   1.416    8089    6893
    2   -6.8  0.0344   1.026 - 1.355   0.940 - 1.134   1.438    4053    3367
    3   -6.8  0.0384   0.808 - 1.451   0.899 - 1.034   1.477    3885    3307
Ratio of minimum to maximum apparent transmission: 0.792922

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Bedford  
  Local Code   MB276A  
  Formula   C38H39ClO2P2Pd  
  Crystal Colour    Colourless  
  Crystal Habit    Prism  
  Crystal Size   0.34 x 0.2 x 0.2 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      SampleCode.hkl - data corrected using  SADABS
      SampleCode_merge_none.hkl - equivalents and friedels kept separate  (See "Final Data Set" table in this report)
      SampleCode.p4p - skeleton p4p file for use with XPREP
      SampleCode.htm - this summary file


Southampton CIF entry fields

_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 

Software References

Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an Obstinate List of Reflections. Journal of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from area-detector images. Journal of Applied Crystallography 2000; 33: 893-898.

Diffractometer control and strategy calculation using COLLECT:
Hooft RWW. COLLECT data collection software, Nonius B.V., 1998.

Standard Data Reduction using HKL(Denzo & Scalepack):
Otwinowski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt A. 1997; 276: 307-326.

Absorption Correction
Sheldrick, G. M. (2003). SADABS. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA.

Non-Standard Data Reduction using EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity evaluation method: EVAL-14. Journal of Applied Crystallography 2003; 36: 220-229.

For more information visit the service web site at: http://www.soton.ac.uk/~xservice/